Transmission electron microscopy has been used to investigate the morphological development of the perovskite (P-) Ti3AlC carbides in the γ matrix of a Ti-45Al-5Nb-0.75C alloy during annealing. P-Ti3AlC carbides in the γ matrix initially have a needle-like shape but during annealing at 800 °C they change to a plate-like shape. In the needle-like shape the carbides are orientated parallel to the [001] direction of the matrix. They extend along the [100]γ or [010]γ direction into plates later and subsequently split into sub particles after extended annealing. It is proposed that the elastic interaction energy between the split sub domains may be the reason that this decomposition into sub-particles is energetically favorable.

Deformation behavior of MoSi2 has been studied by micropillar compressions of single crystalline specimens prepared by focused ion beam (FIB) technique as a function of crystal orientation at room temperature. Activation of the {011}<100> and {01$\overline 3$}<331> slip systems were observed in the micropillars compressed along [$\overline 1$10] and [0 15 1], respectively. The CRSS values for each slip system exhibit an approximate power law relationship with the edge length of micropillar. The {01$\overline 3$}<331> slip exhibit much stronger size-dependence than the {011}<100> slip system.

Molybdenum silicides and borosilicides are promising structural materials for advanced power plants. A major challenge, however, is to simultaneously achieve high oxidation resistance and acceptable mechanical properties at high temperatures. For example, molybdenum disilicide (MoSi2) has excellent oxidation resistance and poor mechanical properties, while Mo-rich silicides such as Mo5Si3 (called T1) have much better mechanical properties but poor oxidation resistance. One approach is based on the fabrication of MoSi2−T1 composites that combine high oxidation resistance of MoSi2 and good mechanical properties of T1. Another approach involves the addition of boron to Mo-rich silicides for improving their oxidation resistance through the formation of a borosilicate surface layer. In particular, Mo5SiB2 (called T2) phase and alloys based on this phase are promising materials.

In the present paper, MoSi2−T1 composites and materials based on T2 phase are obtained by mechanically activated self-propagating high-temperature synthesis (MASHS). To obtain denser products, the so-called SHS compaction (quasi-isostatic pressing of hot combustion products) has been employed. Thermal analysis has shown that SHS compaction significantly improves the oxidation resistance. Self-sustained combustion of Mo/Si/B mixtures for the formation of T2 phase becomes possible if the composition is designed for adding a more exothermic reaction of MoB formation. These mixtures exhibit spin combustion. Oxidation resistance of the obtained multi-phase Mo−Si−B materials is independent on the concentration of Mo phase in the products. The “chemical oven” technique has been used to obtain a single Mo5SiB2 phase and an alloy consisting of α-Mo, Mo5SiB2, and Mo3Si phases.

Half-Heusler MNiSn (M=Ti, Zr, Hf) compounds are well-known, excellent n-type thermoelectric materials. The n-type Seebeck coefficients of ZrNiSn are reduced because of the precipitation of the metallic Heusler ZrNi2Sn phase. An excellent n-type Seebeck coefficient can be converted to p-type based on the vacancy site occupation by the solute Co atoms in the half-Heusler TiNiSn phase as well as ZrNiSn. The Heusler phase precipitates, including their precursor nano-structure in the half-Heusler matrix and the vacancy site occupation of the half-Heusler phase, are regarded as lattice defects based on the crystallographically and thermodynamically close relationship between half-Heusler and Heusler phases.

Periodically arrayed rows of fine Fe2Hf Laves phase particles were found to form in 9Cr ferritic steel. Microstructural observation demonstrates that the particles were formed on cooling through the interphase precipitation on the phase transformation from the δ ferrite to the γ austenite along the eutectoid transformation route of δ → γ+Fe2Hf and subsequently a phase transformation from the austenite to the α ferrite took place. This eutectoid route is expected to be effectively used for improving the long term creep strength of ferritic steels with Laves phase.

The nucleation, growth and coarsening of carbides is investigated in high niobium containing TiAl alloys by diffraction and transmission electron microscopy. Higher carbon content increases the dissolution temperature of carbides. The solubility of carbon is much higher in a γ/α2-phase alloy than in the γ phase alone. Hereby no significant influence of Nb on carbon solubility is found. Crystallographic defects as grain boundaries and dislocations promote carbide nucleation which results in a carbide precipitation sequence starting first at grain boundaries, then at dislocations and only later in the γ matrix away from crystallographic defects. The consumption of carbon by grain boundary carbides or neighboring α2 grains also generates a precipitate free zone in γ grains near the grain boundary.

NiAl, YCu and TiAl polycrystals with B2 and L10 structure, respectively, have been deformed by high pressure torsion (HPT) at temperatures between 20°C and 500°C at a hydrostatic pressure of 8 GPa to high shear strains. Local texture measurements were done by diffraction of high-energy synchrotron radiation and X-ray microdiffraction. In addition, the microstructure was analyzed by electron backscatter diffraction (EBSD). Besides typical shear components an oblique cube component is observed with quite large rotations about the transverse direction. Based on the temperature dependence of this component as well as on microstructure investigations it is concluded that it is formed by discontinuous dynamic recrystallization. The influence of high pressure on recrystallization of intermetallics at low temperatures is discussed.

Ensuring microstructural stability under technical relevant conditions is a determining criterion for the development of innovative high-temperature materials. In this work, the influ-ence of C and Si on the microstructural stability during creep exposure was investigated for a β-solidifying γ-TiAl based alloy with a nominal composition of Ti-43.5Al-4Nb-1Mo-0.1B (in at.%), named TNM. With a two-step heat treatment a microstructure consisting of fine lamellar α2/γ-colonies, surrounded by βo-phase and areas of discontinuous precipitation, starting from the boundaries of the lamellar colonies, was adjusted. Creep tests were carried out to examine the potential of C and Si to prevent microstructural instability during creep and hence improving the creep properties. At 815 °C the discontinuous precipitation process of the TNM alloy continues during ensuing creep testing leading to a reduced creep resistance. In comparison, the minimum creep rate of the TNM-0.3C-0.3Si alloy was significantly decreased caused by the lower βo-phase content and average lamellar spacing within the α2/γ-colonies, the precipitation of p-Ti3AlC carbides and the retarded kinetics of discontinuous precipitation.

The effect of Ti addition on the density and microstructure development of MoSiBTiC alloy was investigated. Two kinds of MoSiBTiC alloys with the composition of Mo-5Si-10B-10Ti-10C (10Ti alloy) and Mo-5Si-10B-15Ti-10C (15Ti alloy) (at. %) were prepared by conventional arc-melting. The primary phase of as-cast 10Ti and 15Ti alloys was (Ti,Mo)C, and there were two eutectic phases of Moss + (Ti,Mo)C and Moss + T2 + (Ti,Mo)C in the alloys. In addition, 10Ti alloy had a Moss + T2 + (Mo,Ti)2C eutectic. There was no Moss + T2 + (Mo,Ti)2C eutectic in the 15Ti alloy, and thus it is apparent that the (Mo,Ti)2C formation was suppressed by 5 at. % Ti addition. The volume fraction of (Ti,Mo)C increased and thus the density reduced from 8.78 to 8.43 g/cm3 with the Ti addition. In all constituent phases, Ti concentration increased while Mo concentration decreased. In spite of the changes, hardness, Young’s modulus and shear modulus were hardly changed. Therefore, Ti addition seems to be effective to further lower the density without deteriorating mechanical properties of the MoSiBTiC alloy.

The crystal structure of the δ1p phase in the Fe-Zn system has been refined by single-crystal synchrotron X-ray diffraction combined with ultra-high resolution scanning transmission electron microscopy. The crystal structure can be described to build up with Fe-centered Zn12 icosahedra. The deformation properties obtained by single-crystal micropillar compression tests of the δ1p phase is discussed in terms of the arrangement of the Fe-centered Zn12 icosahedra in contrast with the ζ phase in the Fe-Zn system.

Three phase Mo-Mo3Si-Mo5SiB2 alloys possess excellent mechanical properties over a wide temperature range. The Mo solid solution phase is needed for balanced mechanical properties at room temperature. However, this phase suffers from catastrophic oxidation behavior at high temperatures caused by the formation and evaporation of MoO3. The oxidation resistance of three phase alloys benefits from a high volume fraction of intermetallic phases. In particular Mo5SiB2 leads to the formation of a borosilicate protective glassy layer on the material’s surface while exposed to air at elevated temperatures. Hence, it is unlikely to identify alloy compositions that will yield both optimum mechanical and oxidation performance.

Different coating systems and techniques, such as pack cementation, magnetron sputtering and plasma spraying are discussed in the literature to control the oxidation properties of Mo-based alloys. A different approach is to apply coating systems based on polymer derived ceramics (PDCs). Our present work introduces PDCs as a new type of promising and innovative oxidation-protective coatings for high temperature Mo-based alloys. After dip-coating with perhydropolysilazane (PHPS) and pyrolysis at 800 °C, dense and well-adhered SiNO ceramic layers could be achieved. These were investigated by scanning electron microscopy. Cyclic oxidation tests at 800 °C and 1100 °C were performed to investigate mass changes due to the thermal treatment. Indeed, even thin pyrolyzed PHPS layers with a thickness of around 70 nm to 175 nm protected the Mo-Si-B substrate during the initial stage of oxidation. By increasing the silicon oxide concentration at the material’s surface a first oxidation barrier was provided and thus, the strong initial mass loss could be decreased as compared to uncoated alloys. Furthermore, first results of the ongoing optimization process on PDC-coatings applied to Mo-Si-B alloys will be presented, involving the enhancement of the coating´s thickness or varying pyrolysis atmospheres.

In the present study, the crystallographic features of bcc/T1/T2 three-phase microstructure in a directionally solidified Mo–32.2Nb–19.5Si–4.7B (at.%) alloy have been examined by electron back-scattering diffraction (EBSD) analysis. The alloy was directionally solidified using an optical floating zone (OFZ) furnace in a flowing Ar gas atmosphere at a constant growth rate of 10 mm/hour. The microstructure of the directionally solidified alloy is characterized by an elongated T2 phase surrounded by inclusions of bcc and T1 phases with an interwoven morphology. The T2 grains are faceted on the (001) planes and elongated along the [110] direction. The T2 phase has an orientation relationship of (001)T2 // (011)bcc and [130]T2 // [2${\rm{\bar 1}}$1]bcc with the bcc phase, whereas any particular orientation relationships of T1 phase with bcc and T2 phases have not been found. These crystallographic features of bcc/T1/T2 three-phase microstructure suggest that the primary T2 phase crystallizes and grows along the [110] direction in liquid phase, followed by nucleation of the bcc phase on the interface between T2 and liquid phases, resulting in bcc/T1 two-phase eutectic reaction surrounding the elongated T2 phase.

Microstructures and mechanical properties of directionally solidified (DS) MoSi2 / Mo5Si3 / Mo5Si3C ternary eutectic composites were investigated. Ternary eutectic microstructure of a script-lamellar type that is characterized by rod-shaped Mo5Si3 and Mo5Si3C phases extending along the growth direction in the MoSi2 single crystalline matrix was developed simply by directional solidification at a growth rate of 10 mm/h. Compression tests along $[{\rm{1}}\mathop 1\limits^- 0]_{MoSi_2 }$ nearly parallel to the growth direction revealed that the DS ternary eutectic composites were plastically deformed above 1000 °C. Yield stresses of the DS ternary eutectic composites were much higher than those of binary composites mainly because of a smaller average thickness of MoSi2 matrix.

To decrease the amount of precious metal usage for Pd-catalyzed aerobic alcohol oxidation, various amount of Cu-contained Pd bimetallic nanoparticle-supported solid base hydrotalcite catalyst (PdxCuy-PVP/HTs) were prepared and applied for aerobic benzyl alcohol oxidation. It was found that the addition of Cu atoms into Pd in the range of 0-40% provided a similar or a little superior activity to that of Pd100-PVP catalyst, whereas a large quantity of co-existence Cu (>40%) gradually decreased their activity of the catalyst. The aerobic benzyl alcohol oxidation over Pd80Cu20-PVP/HT served 77% yield and 95% selectivity towards benzaldehyde at 313 K for 5 h in toluene under O2 flow. X-ray adsorption spectroscopy (XAS) studies and scanning transmission electron microscopy-high angle annuar dark field (STEM-HAADF) with energy dispersive X-ray spectroscopy (EDS) analyses suggested that Cu atoms doping into Pd(0) NP influenced not only localized nanostructure but also oxidation state around Pd atoms. We suggested that substitution of precious metal with small amount of transition metals such as Cu lead to geometric/electronic changes in active sites would be one of nice strategies for reducing the cost for the catalyst in the oxidation process.

New low aluminium high niobium TiAl alloys exhibit a nano scale modulated microstructure consisting of lamellae with a tweed substructure. These tweed like appearing lamellae are a modulated arrangement of at least two phases. One constituent of the crystallographic modulation in the lamellae is an orthorhombic phase, which is closely related to both the hexagonal α2-Ti3Al phase and the cubic B2 ordered βo-TiAl phase.

In this study the nature and formation of this orthorhombic phase has been investigated by high-energy X-ray diffraction.

Measurements have shown that the newly formed orthorhombic phase is structurally comparable to the O phase (Ti2AlNb). It forms in the temperature range of 550 °C to 670 °C from the α2 phase by small atomic displacements and chemical reordering. The in situ experiments yielded information about the thermal stability of the orthorhombic phase. After dissolving at temperatures above 700 °C the phase can be re-precipitated by annealing within the temperature range of formation.

The formation frequency of habit plane variant (HPV) clusters in Ni-25Pd-50Ti shape memory alloy was analyzed using electron backscattering diffraction (EBSD) on the basis of the geometrically nonlinear theory of martensite. Two types of cluster, diamond and wedge, were most commonly observed. The ratio of the formation frequency of the diamond to wedge clusters was approximately 1 : 3, whereas the rotation to keep the kinematic compatibility (KC) condition, θ *, was 3.9° and 0.0032°, respectively. The ratio of the formation frequency is quantified by the value of θ * which is an indicator of the incompatibility of the cluster. The origin of the diamond cluster is discussed based on the degree of incompatibility.

The effect of W addition on microstructure and mechanical properties of Ni3Al (L12) and Ni3V (D022) two-phase intermetallic alloys has been investigated. W was added to the base alloy composition, Ni75Al10V12Nb3 (at. %) in place of either Ni, Al or V. The W-added alloy ingots were heat-treated in vacuum at 1575 K for 5 h. The majority of W-added alloys showed a dual two-phase microstructures while the alloy in which 3 at. % W substituted for Ni exhibited the dual two-phase microstructure containing W solid solution dispersions. Vickers hardness was significantly enhanced by W addition, which is primarily due to solid-solution strengthening.

The effect of Si addition on microstructure and mechanical properties of dual two-phase intermetallic alloys was investigated. Si was added to the base alloy composition Ni75Al9V13Nb3 + 50 wt. ppm B by three substitution ways in which Si was substituted either for Ni, for Al and for V, respectively. The alloys added with 1 at.% Si showed a dual two-phase microstructure composed of Ni3Al (L12) and Ni3V (D022) phases, while the alloys added with over 2 at.% Si exhibited the same dual two-phase microstructure but contained third phases. The third phases were G phase (Ni16Si7Nb6) and A2 phase (the bcc solid solution consisting of Nb and V). Yield and tensile strength of the 1 at.% Si-added alloys were high in the alloy in which Si was substituted for Al but low in the alloys in which Si was substituted for Ni or for V, in comparison with those of the base alloy. Tensile elongation was lower than that of the base alloy irrespective of substitution ways. The density of the Si added alloys was close to or slightly lower than that of the base alloy. Oxidation resistance of the Si added alloy was increased. Si addition to the dual two-phase intermetallic alloys is beneficial for reducing the density and enhancing the oxidation resistance without a harmful reduction of strength properties.

A micro-sized fracture testing method has been applied to investigate fracture toughness of alpha-Nb5Si3. Chevron-notched single crystal specimens with a size of 3 x 3 x 15 μm3 were prepared in a grain of polycrystalline alpha-Nb5Si3 by focused ion beam, FIB, technique. Fracture tests were conducted using a nanoindenter at room temperature and linear load-displacement curves and smooth fracture surfaces were obtained. This fracture behavior was presumed to be brittle fracture similar to bulk alpha-Nb5Si3. The average of fracture toughness KQ is 3.45 ± 0.29 MPa√m under a small-scale yielding condition.

In this work we examine a Ti-48Al-2Cr-2Nb alloy obtained with an additive manufacturing technique by Electron Beam Melting (EBM) by conducting monotonic and cyclic loading experiments both on tension and compression samples for investigating the influence of the microstructure in strain accumulation process by fatigue loading. The residual strain maps corresponding to different applied stress levels, number of cycles and microstructures are obtained through the use of high-resolution Digital Image Correlation (DIC). The strain maps were overlaid with the images of the microstructure and detailed analyses were performed to investigate the features of the microstructure where high local strain heterogeneities arise. Such experiments, conducted ex-situ at room temperature, allow to characterize the effect of different microstructures on the strain accumulation process, and to clearly identify the role of the microstructural features of this TiAl intermetallic alloy on the fatigue initiation process.